The unique properties of supercritical fluids (SCFs) have been widely used since the 1980’sin a wide range of applications including separation, chemistry and materials synthesis.Currently, the research activities are focused toward a better understanding and tailoring ofthermodynamical, physical and chemical phenomena involved in SCFs processes. In thiscontext, this is why we have chosen to develop supercritical microfluidics in the frame of thisPhD work, which aims at developing and using microfluidic tools in order to study the chemicalreactivity and the nucleation-growth in supercritical fluids.First of all, our strategy aimed at fabricating microsystems which could handle to the SCFsoperating conditions (high pressure and high temperature). Then, we have studied somephysical characteristics of these devices and in particular we determined the expectedadvantages associated with the combination of microfluidic tools and supercritical fluids.Afterwards, we have demonstrated the benefits of the supercritical microfluidics to materialssynthesis and chemical reactivity through the hydrothermal oxidation of methanol and thesynthesis of ZnO nanocrystals. This last point was also the subject of a photoluminescencestudy, demonstrating that supercritical microfluidics tools can be used as “precision synthesis”reactors.